Filter powder



Patented Dec. 11,- 19 45 UNITED STATES PATENT OFFICE Thomas C. Atwell, Warren, Pa, asslg'nor to Florldin Company, Warren, Pa., a corporation of Delaware No Drawing.

Serial No. 591,625

2 Claims. (Cl. 252-299) powder has been disclosed in the Fitz application, Serial No. 273,146, for Filter powder,

7 This invention relates to the preparation of a decolorizing filter aid and more particularly to the treatment of fullers earth to make it useful for this purpose. The application is. a continuation-in-part of my copending application Serial No, 413,369, filed October 2, 1941.

It is an object of the invention to provide a 'fuller's earth decolorizing filter aid having im-' proved fiow rate characteristics while retaining as high an efllciency for decolorizlng and fatty filter aids now available commercially.

It is the particular object of this invention to provide a fullers earth decolorizing filter powder for use in the reclamation of dry cleaning fluids to clarify and purify the solvent fluid for reuse. The principal commercially acceptable solvents used in the dry cleaning field with which the invention is operable are the following:

Stoddard solvent-a petroleum naphtha Carbontetrachloride Trichloroethylene Tetrachloroethylene (perchloroethylene) 140 F. flash petroleum solvent It is an equally important object of the inven-,

- tion to provide a decolorizing filter aid which has properties of both an adsorbent and a filter aid, and can be used to treat the following industrial liquids in addition to dry cleaners solvent:

Animal, vegetable, and mineral oils Shellac Metallurgical solutions Adhesives Cellulose esters Pharmaceuticals Fruit juices Cider Alcoholic extracts and many others wherever filter aid action, clan.-

acid adsorption characteristics as fullers, earth Simona filed May 11, 1939. As there shown, the fullers earth may be crushed and dried to remove all of the free and adsorbed moisture and is further dried to have a water of hydration content less than 6% but not less than 1%. The dried fullers earth is then subjected to a fine grinding process during which it is pulverized to have a particle size range below '74 microns. It has been found that fullers earth thus treated has superior decolorizing and fatty acid adsorption characteristics which render it particularly adapted to the reclamation of dry cleaning solvent fluids, though it is also contemplated that such a material may be used for many other purposes.

Fuller's earth processed in this manner is well adapted to this dry cleaning use, because, when the tullers earth is activated by reducing its water of hydration content to not less than 1% and less than 6%, it is rendered impervious to subsequent swelling when water entrained with the solvent fication, neutralization, or decolorization can be applied.

The present invention makes available various fullers earths; e. g., the Georgia-Florida. type, the Texas type such as obtained from Riverside, Texas, the Olmstead, Illinois type, and others to accomplish the purposes of filter powders and imparts to the same characteristics which enable the filter aid may be disground fullers earth filter contacts the filter powder. Thus, the filter aid collected on a screen will permit the dry cleaning fluid to pass readily therethrough, unimpeded by the usual swelling and gelatinization which normally follows from the use of fullers earth in the presence of moisture. Once dried to this water of hydration content, the fullers earth may be placed in contact with water without detrimental swelling or gelatinization.

While the fullers earth filter powder above described has superior characteristics in the respects named, improvement in the flow rate of the solvent through the powder collecting on the screen is accomplished by'following the steps to be described below.

Flow rate is defined as the quantity of liquid I passing through a unit area of the filter aid, per unit thickness per unit pressure differential in a given time. By treating the fullers earth in the manner of this invention, the flow rate characteristic can be improved materially while, at the same time, retaining its other above-described characteristics as a filter aid.

It is preferred that in addition to or treating the fuller's earth here described, that the earth. be activated in accordance with the teaching of the co-pending application. This invention is an improvement on that disclosure.

and resides in controlling the fine grinding process to control the particle size of the filter aid. It has been found that flow rate is dependent on particle size particularly where thereare large percentages of fines smaller than 10 microns. It is the purpose of this invention to provide a method of grinding whereb the proportion of fines may be reduced, so that notwithstanding that all of the fullers earth is ground to a particle size 1 smaller than 74 microns. the distribution of parthe process ticle sizes may be controlled to eliminate most of the fines in the ground product less than 10 microns in diameter. The resistance to flow of fluid through the filter powder is inversely proportional to the quantity and size of the fines in the powder. The fewer the fines and narrower the classification, i. e., particle diameter limit, the less will be the resistance. It is apparent, therefore, that the fines should be eliminated to improve the fiow rate.

The size or the particles obtained in the fine grinding process is related to the brittleness, the

shattering characteristics, and the toughness of the fullers earth being pulverized. These qualities I find are dependent to a certain extent upon the natural free and combined water content of the fullers earth, and if the free water content is controlled while the fine grinding process is accomplished, the particle size of the finished product may be made to fall within a certain range. The tendency of the earth to pulverize to a uniform particle size will be found to vary with the variation in the selected quantity of natural free water.

If fullers earth having a. critical natural free water content of between substantially 20 to 40% is subjected to grinding, for example in a Raymond plant size roller mill or other conventional grinding equipment such as a hammer mill or a grinder in which the material is pulverized by feeding it between a stationary disc and a. revo1v-' ing disc, a filter aid results, having an improved 'fiow rate, by reason of the elimination of a sub- The optimum free water content is within the range of 20% to 40% natural free moisture content. This rahge tends to produce the most uniform size'in the final product and reduces to a minimum the proportion of fines produced in the pulverizlng means. Below 20% free moisture, the

proportion of fines tends to increase and the flow rates are so low that the ground earth is of no commercial value.

The criticality of the substantially 20 to 40% free water content is illustrated in the following table showing the efiect of free moisture. content on flow-rate in the present invention:

Table 1 Per cent tree Flow-rate water at ocJ'min. overtime of age of four grinding test runs 9. 4 5 l3. 6 10 an. a e 81. 2 2) 48.0 70. 8 so 104 86 140 40 F 10! 'i o'o hetieto d. All rates onggter. All sampler ground to 200 mesh lndneflratedat 800' F. The value are the average of tomdiilerent runs.

In the above table the free moisture content I g .15 have a water of hydration content of not less tame has been extendedto the limits of grind ability which from the table is about 40% free water. It will be noted that the flow-rate increases sharply above 20% free water and continues to rise up to the limit 01' about 40%. The

5 lower limit of 20% is fixed, due to the fact that the fiow rates resulting below this limit are com- I mercially of no value and the upper limit of about 40% is fixed, because at this point the clay becomes plastic and sticky so that it cannot be 10 ground.

To obtain a fullers earth having 20% to 40% free moisture content, the earth is dried at a temperature below about 250 F. If heated above this degree, a portion of the combined water of '15 hydration will be driven ofi and the'earth upon then being ground will have an undue proportion of fines. After grinding to obtain the desired particle size distribution, in accordance with this teaching, the earth. is activated by drying 20 it to a combined or water of hydration content of not less than 1% and less than 6%, so that in addition t the improved flow rate thus obf tained, all of the useful properties of the activated fullers earth of the prior artare preserved.

5 In the preferred practice of this invention, the

raw fuller's earth is subjected to a crushing step to produce a somewhat uniform size of lump. The fullers earth passes from the primary swing hammer crushing mill to a rotary drier where 30 the fullers earth is subjectedto the drying temperature, which is below about 250 F., until the free moisture content of the-earth is reduced to within the 20% to 40% range. The fullers earth is then pulverized to a particle sizebelow '74 35 microns, as, for example, with a Raymond mill.

The Raymond mill is the well-known type of pulverizing apparatus in which the material to be pulverized is fed downwardly into a receptacle having a stationary and horizontally dis-.

40 posed grinding ring against the inner periphery of which grinding rollers are forced. The grinding rollers are rotatably mounted on the ends of vertically extending shafts which, in turn, are pivotally mounted on a spider driven by a vertical drive shaft. As the drive shaft is rotated,

the inner periphery of the grinding ring and will be forced outwardly by centrifugal force to crush the material between the rollers and the ring. A

blast of air is forced upwardly through the ground material, and, as the air stream continues upwardly, it passes through an enlarged chamber where its velocity is greatly reduced, whereby the heavier'particles are returned to the grinding means and only the lighter particles are carried over to the further classifying and collecting means. 1

-When fuilers earth, dried to within a range of 20% to 40% natural free moisture, is thereof mill, 9. more uniform particle size and a narrower classification results than if it were ground at a'lower moisture content. Due to the control of the natural free moisture content, the

o5 fuliers earth can be ground to a size range bethe crushing rollers will be caused to roll around after subjected to the grinding step in any yp I the performance of fine 'oi colloidal-fines, a

than 1% and less than 6% after the fine grinding has been periormed.

It is desirable in the finished product to be used in the dry cleaning arts that all particles of colloidal size be removed. If not removed, the

' colloidal particles adhere to the fabrics being cleaned and cause an increase in resistance to fiow of .fiuid through the filter device. Although V grinding practice as here taught tends to eliminate the production small proportion of the ground material will be of this size, and thus all fines smaller than 3 microns should be removed. a

A typical analysis of a tuller's earth ground in accordance with the present invention (sample A), as compared with the prior art teachins wherein the' free moisture content was disregarded in the fine grinding state (sample B),

From an inspection of this analysis, it is evidentthat th fuiler's earth sample A which was dried to have a free moisture content of 20% to 30% before fine grinding has a much'larger percentage of larger sized particles than the fullers earth sample B which was pulverized after the moisture content had been reduced to 1% to 6% water ofhydration. It will be noted that sample A has a size range in which over 67% of the particles are larger than 10 microns. Sample B has a much larger proportion of fines, and it will be noted that only has a particle size larger than .10 microns. It is this elimination of the fineswhich accounts for the larger flow rate, 146 cc./min. per unit area per unit thickness per pressure difierential per unit time, as compared with "17 cc./min. for sample B.

In following the present teaching, it is possible to produce a powder having 80% within the particle size range of 10 to 25' microns. A powder having this size range with 100% below 74 m1- crons, has an average flow rate of 160 cc./min. The tremendous gain in flow rate accomplished by this invention is of important comm value. in that it enables the flow rate to increase aseoaoo poses. That is,

perior product will be substantially over that formerly obtained; e. g., 3 to 5 times or more.

It has been stated that the fuller's earth thus processed is useful for other purposes, and it is suggested that by following the dry grinding process here described and the activation step set forth in the Fitz Simons application, that a suproduced for a number of other filtering uses, such as for decolorizing oils, removing fatty acids from other liquids not attracted to the filter aid, etc.

In certain of such other uses, activation to not less than 1% and less may not be essential. .This drying is performed, primarily, to improve the filter powder for uses where water comes in contact withfthe powder,

the improvement being the avoidance of swelling or gelatinization when water contacts the powder. i

While I have mentioned Georgia-Florida, Texas, and Olmstead types specifically. I find that the invention is useful generally for the improvement of fullers earths for decolorizing filter powders. and regardless of grinding equipment and the crude earths available, has general application to the preparation of high fiow rate filter powders from fuller's earth.

I have referred herein to the particular utility of the decolorizing filter powder'in the dry cleaning industry. When incorporated in one of the usual solvents, such as above referred to, in which may be also included a detergent such as a soap, the action of' the product of this invention is highly efilcient both as a filter aid and as a decolorizing agent and precludes the necessity for independent or separate mediums for these purthe product of the invention is effective as a filter aid; a purifying and decolorizing agent. For a more complete understanding of of the material erciab and thereafter activat the application of the invention in the dry cleaning field, reference is had to Industrial and Engineering Chemistry," volume 32, page 454, April 1940, in which the customary dry cleaning process and theprovince of the filter powder is fully described.

I claim: 1. A process for dry grinding fullers earth to control the distribution of the particle sizes comprising drying the raw earth to have a natural freemoisture content of between about 20% to I 40%, then grinding the dried earth to a particle size below '14 microns.

2. A process for dry grinding fuller's earth to control the distribution of the particle sizes for use as a decolorizing filter aid in the reclamation of a dry cleaning fluid comprising drying theraw earth to have a-natural free moisture content of between about 20% to 40%, I dried earth to a particle size below '14 microns, ing the earth by drying it to have a water of hydration content of from not less than about 1% to less than 8%.

' a moms c. A'I'WEIL.

than 6% combined water then grinding the I 

